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1.
The crystallization behaviour of amorphous melt spun Fe82?x?yCr18ZrxBy (x=0–8, y=10–20) ribbons have been investigated using differential scanning calorimetry. The crystallization temperature and crystallization behaviour change with varzing Zr and B content. The microstructural development during annealing of amorphous Fe64Cr18Zr8B10 has been investigated by a combination of transmission electron microscopy and energy dispersive X-ray microanalysis. Isothermal annealing for 2 h at temperatures in the range 600–1000°C produces a variety of different microstructures depending on the annealing temperature. At 600°C, the amorphous alloy partially crystallizes to a form a microstructure consisting of 9 nm sized bee ferrite grains embedded in an amorphous matrix. At temperatures in the range 700–900°C, the alloy microstructure transforms into a mixture of bee ferrite, faulted fcc MB12 boride particles and tetragonal M3B boride particles. At 1000°C, the faulted fcc MB12 boride particles are replaced by orthorhombic M4B boride particles.  相似文献   

2.
B/Nb and B/Nb2N bilayers and Nb/B/Nb trilayers of about 550 nm total thickness have been deposited on Si(100) wafers with 100 nm thermally grown oxide. Nb and B layers were deposited by magnetron sputtering. Nb2N layers were prepared by nitridation of Nb films via rapid thermal processing (RTP). The samples were annealed subsequently at temperatures between 600 and 1,200 °C in an RTP system under Ar or NH3 gas flow to study interdiffusion and reactivity of niobium, boron and nitrogen. Formation of phases was investigated by X-ray diffraction (XRD); surface morphology and roughness were studied via scanning electron microscopy (SEM) and atomic force microscopy (AFM), respectively. Elemental depth profiles of selected samples were recorded by secondary ion mass spectrometry (SIMS). Annealing of the B/Nb bilayers and Nb/B/Nb trilayers under Ar leads to the formation of Nb3B2 at 1,200 °C at the B/Nb interface. At lower temperatures the high oxygen content in the boron layer is supposed to hinder the formation of borides due to formation of glass-like boron oxides. In NH3 several niobium nitrides are formed but no boride phases. Here again the reactivity of boron with niobium is suppressed by the high oxygen content and boron oxide formation. During annealing of the B/Nb2N bilayers no borides were formed indicating that well-formed Nb2N is an effective diffusion barrier for B.  相似文献   

3.
The Perthioborates RbBS3, TIBS3, and Tl3B3S10 . RbBS3 (P21/c, a=7.082(2) Å, b=11.863(4) Å, c=5.794(2) Å, β=106.54(2)°) was prepared as colourless, plate-shaped crystals by reaction of stoichiometric amounts of rubidium sulfide, boron, and sulfur at 600°C and subsequent annealing. TlBS3 (P21/c, a=6.874(3) Å, b=11.739(3) Å, c=5.775(2) Å, β=113.08(2)°) which is isotypic with RbBS3 was synthesized from a sample of the composition Tl2S · 2 B2S3. The glassy product which was obtained after 7 h at 850°C was annealed in a two zone furnace for 400 h at 400→350°C. Yellow crystals of TlBS3 formed at the warmer side of the furnace. Tl3B3S10 (P1 , a=6.828(2) Å, b=7.713(2) Å, c=13.769(5) Å, α=104.32(2)°, β=94.03(3)°, γ=94.69(2)°) was prepared as yellow plates from stoichiometric amounts of thallium sulfide, boron, and sulfur at 850°C and subsequent annealing. All compounds contain tetrahedrally coordinated boron. The crystal structures consist of polymeric anion chains. In the case of RbBS3 and TlBS3 nonplanar five-membered B2S3 rings are spirocyclically connected via the boron atoms. To obtain the anionic structure of Tl3B3S10 every third B2S3 ring of the polymeric chains of MBS3 is to be substituted by a six-membered B(S2)2B ring.  相似文献   

4.
Systematic studies on selenoborates containing a B12 cluster entity and alkali metal cations led to the new crystalline phase Na6[B18Se17] which consists of a icosahedral B12 cluster completely saturated with trigonal‐planar BSe3 units and sodium counter‐ions. Neighbouring cluster entities are connected in one direction via exocyclic selenium atoms forming the infinite chain anion ([B18Se16Se2/2]6–). The new chalcogenoborate was prepared in a solid state reaction from sodium selenide, amorphous boron and selenium in evacuated carbon coated silica tubes at a temperature of 850 °C. Na6[B18Se17] crystallizes in the monoclinic space group C2/c (no. 15) with a = 18.005(4) Å, b = 16.549(3) Å, c = 11.245(2) Å, β = 91.35(3)° and Z = 4.  相似文献   

5.
For the first time perthioborates with trigonal planar coordination of boron were prepared. Na2B2S5 (Pnma, a = 12.545(2) Å, b = 7.441(1) Å, c = 8.271(1) Å, Z = 4) and Li2B2S5 (Cmcm, a = 15.864(1) Å, b = 6.433(1) Å, c = 6.862(1) Å, Z = 4) were obtained by reaction of the metal sulfides with stoichiometric amounts of boron and an excess of sulfur (effective molar ratio M:B:S = 1:1:4) at 600°C (650°C) and subsequent annealing. The non-isotypic structures contain exactly planar [B2S5]2? groups consisting of five-membered B2S3 rings with one additional exocyclic sulfur on each of the boron atoms. The alkaline metal cations are four-coordinate (lithium) and (four + four)-coordinate (sodium) respectively.  相似文献   

6.
Li5B7S13 and Li9B19S33: Two Lithium Thioborates with Novel Highly Polymeric Anion Networks Li5B7S13 (C2/c; a = 17.304(2) Å, b = 21.922(3) Å, c = 12.233(2) Å, β = 134.91(1)°; Z = 8) and Li9B19S33 (C2/c; a = 23.669(9) Å, b = 14.361(3) Å, c = 12.237(3) Å, β = 103.77(2)°; Z = 4) were prepared by reaction of stoichiometric amounts of lithium sulfide, boron, and sulfur at 750°C (Li5B7S13) and 700°C (Li9B19S33) with subsequent annealing. The crystal structures consist of interpenetrating, polymeric boron sulfur anion networks which are formed by corner-sharing of B4S10 and B10S20 units (Li5B7S13), or B19S36 units (Li9B19S33). The lithium cations are situated in between with a strong disorder in Li9B19S33.  相似文献   

7.
Three Novel Selenoborato- closo -dodecaborates: Syntheses and Crystal Structures of Rb8[B12(BSe3)6], Rb4Hg2[B12(BSe3)6], and Cs4Hg2[B12(BSe3)6] The three selenoborates Rb8[B12(BSe3)6] (P1, a = 10.512(5) Å, b = 10.450(3) Å, c = 10.946(4) Å, α = 104.53(3)°, β = 91.16(3)°, γ = 109.11(3)°, Z = 1), Cs4Hg2[B12(BSe3)6] (P1, a = 9.860(2) Å, b = 10.740(2) Å, c = 11.078(2) Å, α = 99.94(3)°, β = 90.81(3)°, γ = 115.97(3)°, Z = 1), and Rb4Hg2[B12(BSe3)6] (P1, a = 9.593(2) Å, b = 10.458(2) Å, c = 11.131(2) Å, α = 99.25(3)°, β = 91.16(3)°, γ = 116.30(3)°, Z = 1) were prepared from the metal selenides, amorphous boron and selenium by solid state reactions at 700 °C. These new chalcogenoborates contain B12 icosahedra completely saturated with six trigonal-planar BSe3 entities functioning as bidentate ligands to form a persubstituted closo-dodecaborate anion. The two isotypic compounds Rb4Hg2[B12(BSe3)6] and Cs4Hg2[B12(BSe3)6] are the first selenoborate structures containing a transition metal which are characterized by single crystal diffraction.  相似文献   

8.
Na2B2Se7, K2B2S7, and K2B2Se7: Three Perchalcogenoborates with a Novel Polymeric Anion Network Na2B2Se7 (I 2/a; a = 11.863(4) Å, b = 6.703(2) Å, c = 13.811(6) Å, β = 109.41(2)°; Z = 4), K2B2S7 (I 2/a; a = 11.660(2) Å, β = 6.827(1) Å, c = 12.992(3) Å, β = 106.78(3)°; Z = 4), and K2B2Se7 (I 2/a; a = 12.092(4) Å, b = 7.054(2) Å, c = 13.991(5) Å, β = 107.79(3)°; Z = 4) were prepared by reaction of stoichiometric amounts of sodium selenide (potassium sulfide) with boron and sulfur or of potassium selenide and boron diselenide, respectively, at 600°C with subsequent annealing. The crystal structures consist of polymeric anion chains of composition ([B2S7]2?)n or ([B2Se7]2?)n formed by spirocyclically connected five-membered B2S3 (B2Se3) rings and six-membered B2S4 (B2Se4) rings. The nine-coordinate alkaline metal cations are situated in between.  相似文献   

9.
The temperature dependence of the volume fraction of the crystalline phase in Fe80B20 amorphous alloy is calculated using equations from the homogeneous nucleation theory of binary systems. It is shown that the crystallization of Fe80B20 alloy is two-stage, as is confirmed by the experimental data obtained by means of highly sensitive dilatometry and X-ray diffractometry. On the basis of results of calculations performed within the theory of the high-temperature stability of amorphous alloys, two areas of its practical application are proposed: (i) enhancing the thermal stability of amorphous alloys by isothermal annealing in the range of temperatures where crystalline nuclei can transition to the amorphous phase; (ii) controlled nanostructuring of the amorphous state with different modes of treatment. Methods are proposed for obtaining the nanostructured state from the initial amorphous state. Alloys in the nanocrystalline state are obtained, as is confirmed by the results from electron microscope investigations.  相似文献   

10.
Gd10I16(C2)2 and Gd10Br15B2/Tb10Br15B2 Cluster Compounds with M10 Twin Octahedra The compound Gd10I16(C2)2 can be prepared from Gd metal, GdI3 and C at 950 °C. It crystallizes in P1 with a = 10.463(4) Å, b = 16.945(6) Å, c = 11.220(4) Å, α = 99.15(3)°, β = 92.68(3)° und γ = 88.06(3)°. Gd10Br15B2 is formed between 900 und 950 °C, Tb10Br15B2 between 900 und 930 °C from stoichiometric amounts of the rare earth metals, tribromide and boron. Both compounds crystallize in the space group P1 for Gd10Br15B2 with a = 8.984(2) Å, b = 9.816(2) Å, c = 10.552(5) Å, α = 91.14(3)°, β = 114.61(3)° and γ = 110.94(3)° and for Tb10Br15B2 with a = 8.939(4) Å, b = 9.788(3) Å, c = 10.502(2) Å, α = 91.19(3)°, β = 114.51(3)° and γ = 111.10(2)°. In the crystal structures of all three compounds the rare earth metals form edge‐shared Ln10 twin octahedra. In Gd10I16(C2)2 the Gd octahedra are centered with C2 groups (dC–C = 1.43(7) Å). In Ln10Br15B2 (Ln = Gd, Tb) the octahedra contain single boron atoms. The clusters are connected through halide atoms to chains [Ln10(Z)2X X X ]. Adjacent chains are fused threedimensionally via I I for the Gd iodide carbide and via Br Br for the bromide borides of Gd und Tb. It is interesting to see an identical pattern of connection between the chains for the reduced oxomolybdates, e. g. PbMo5O8.  相似文献   

11.
WO3 films have been prepared onto IrO2-coated Ti substrate by electro-deposition, and as-deposited and annealed films have been characterized by using Raman spectroscopy. It was found that the asdeposited film consists of orthorhombic WO3 · H2O phase, which transforms to amorphous WO3 by annealing at 250°C and to monoclinic phase by annealing at and above 350°C. All electrochemical experiments were carried on Ti/IrO2/WO3 annealed at 450°C. The open-circuit potential could change significantly due to the hydration of the coating film. However this process is fairly slow. Reproducible voltammograms could be obtained quickly, further revealing high electrochemical stability of the Ti/IrO2/WO3 electrode. And the shapes of CV show the approximate rectangular mirror image, showing the typical characteristic of capacitive behavior. The specific capacitance obtained at a scan rate of 50 mV s−1 is 46 F g−1.  相似文献   

12.
Cs2B2S4 – A Derivative of the Dimeric Metathioboric Acid Cs2B2S4 (structure: I41/acd; a = 7.270(1) Å, c = 35.737(7) Å; Z = 8; substructure: I4/mmm; a′ = 5.141(1) Å, c′ = 17.868(4) Å, Z = 2) is prepared by the reaction of cesium sulfide with stoichiometric amounts of boron and sulfur (effective molar ratio M:B:S = 2:2:4) at 600°C and subsequent annealing. The crystal structure contains isolated [B2S4]2? groups consisting of four-membered B2S2 rings with two exocyclic sulfur atoms on each of the boron atoms. The cesium cations are nine-coordinate between these rings. The structural feature of two edge-sharing BS3 groups forming an isolated anion appears for the first time in thioborate chemistry, although it is known as a part of the polymeric network in B2S3.  相似文献   

13.
Spherical magnetic Mg-Fe-O nanoparticles were successfully prepared by the crystallization of glass in the system K2O/B2O3/MgO/P2O5/Fe2O3. The magnetic glass ceramics were prepared by melting the raw materials using the conventional melt quenching technique followed by a thermal treatment at temperatures in the range 560–700 °C for a time ranging from 2 to 8 h. The studies of the X-ray diffraction, electron microscopy and FTIR spectra confirmed the precipitation of finely dispersed spherical (Mg, Fe) based spinel nanoparticles with a minor quantity of hematite (α-Fe2O3) in the glass matrix. The average size of the magnetic nano crystals increases slightly with temperature and time from 9 to 15 nm as determined by the line broadening from the XRD patterns. XRD studies show that annealing the glass samples for long periods of time at temperature ≥604 °C results in an increase of the precipitated hematite concentration, dissolution of the spinel phase and the formation of magnesium di-borate phase (Mg2B2O5). For electron microscopy, the particles were extracted by two methods; (i) replica extraction technique and (ii) dissolution of the glass matrix by diluted acetic acid. An agglomeration of the nano crystals to larger particles (25–35 nm) was observed.  相似文献   

14.
Phosphoraneiminato Complexes of Boron. Syntheses and Crystal Structures of [BBr2(NPMe3)]2, [B2Br3(NPiPr3)2]Br, [B2(NPEt3)4]Br2, [B2Br2(NPPh3)3]BBr4 and [{B2(NMe2)2}2(NPEt3)2]Cl The bromoderivatives of the title compounds are prepared from the corresponding silylated phosphoraneimines Me3SiNPR3 and boron tribromide. The boron subcompound [{B2(NMe2)2}2(NPEt3)2]Cl2 derives from Me3SiNPEt3 and B2Cl2(NMe2)2. All complexes are characterized by NMR and IR spectroscopy as well as by crystal structure determinations. [BBr2(NPMe3)]2 (1): Space group P21/n, Z = 2, R = 0.031. Lattice dimensions at ?50°C: a = 723.8, b = 894.2, c = 1305.4 pm, β = 92.35°. 1 forms centrosymmetric molecules in which the boron atoms are linked via μ2-N bridges of the NPMe3? groups of from B2N2 four-membered rings with B? N distances of 149.9 and 150.9 pm. B2Br3(NPiPr3)2]Br (2): Space group P21, Z = 2, R = 0.059. Lattice dimensions at ?80°C: a = 817.6, b = 2198.7, c = 851.5 pm, β = 115.09°. In the cations of 2 the boron atoms are lined via the μ2-N atoms of the NPiPr3? groups to form planar, asymmetric B2N2 four-membered rings with B? N distances of 143 and 156 pm. [B2(NPEt3)4[Br2·4CH2Cl2 (3): Space group C2/c, Z = 4, R = 0.042. Lattice dimensions at ?50°C: a = 1946.1, b = 1180.3, c = 2311.3 pm, β = 101.02°. The structure contains centrosymmetric dications in which both the boron atoms are lined by the N atoms of two of the NPEt3? groups to form a B2N2 four-membered ring with B? N distances of 149.6 pm. The remaining two NPEt3? groups are terminally bonded with very short B? N distances of 133.5 pm. B2Br2(NPPh3)3]BBr4 (4): Space group P1 , Z = 2, R = 0.065. Lattice dimension at ?50°C: a = 1025.7, b = 1496.1, c = 1807.0 pm, α = 85.09°, β = 82.90°, γ = 82.72°. In the cation the boron atoms are lined via the μ2-N atoms of two of the NPPh3? groups to form a nearly planer B2N2 four-membered ring with B? N distances of 149.3-153.1 pm. The third NPPh33 group is terminally connected with teh sp2 hybridized boron atom and with a B? N distance of 134.1 pm along with an almost linear BNP bond angle of 173.6°. [{B2(NMe2)2}2(NPEt2)2]Cl2 · 3CH2Cl2 (5): Space group C2/c, Z = 4, R = 0.098. Lattice dimensions at ?70°C: a = 1557.9, b = 1294.7, c = 2122.9 pm, β = 96.08°. The structure of 4 contains centrosymmetric dications in which two by two B-B dumb-bells are linked via the μ2-N atoms of the two NEPt3? groups to form B4N2 six-membered rings with B? N distances of 150 and 156 pm and B-B distances of 173 pm. The B? N distances of the terminally bonded NMe2? groups correspond to 138 pm double bonds.  相似文献   

15.
By powder X-ray diffraction the structure of the monoclinic modification of Re3B is studied. The phase is obtained under high pressure and high temperature (10 GPa, 1800°C) using nanocrystalline rhenium and amorphous boron. The results of the comparative crystal chemical analysis are reported.  相似文献   

16.
Li6+2x[B10Se18]Sex (x ≈ 2), an Ion‐conducting Double Salt Li6+2x[B10Se18]Sex (x ≈ 2) was prepared in a solid state reaction from lithium selenide, amorphous boron and selenium in evacuated carbon coated silica tubes at a temperature of 800 °C. Subsequent cooling from 600 °C to 300 °C gave amber colored crystals with the following lattice parameters: space group I2/a (at 173 K); a = 17.411(1) Å, b = 21.900(1) Å, c = 17.820(1) Å, β = 101.6(1)°. The crystal structure contains a well‐defined polymeric selenoborate network of composition ([B10Se16Se4/2]6?)n consisting of a system of edge‐sharing [B10Se16Se4/2] adamantanoid macro‐tetrahedra forming large channels in which a strongly disorderd system of partial occupied Li+ cations and additional disordered Se2? anions is observed. The crystal structure of the novel selenoborate is isotypic to Li6+2x[B10S18]Sx (x ≈ 2) [1]. X‐ray and 7Li magic‐angle spinning NMR data suggest that the site occupancies of the three crystallographically distinct lithium ions exhibit a significant temperature dependence. The lithium ion mobility has been characterized by detailed temperature dependent NMR lineshape and spin‐lattice relaxation measurements.  相似文献   

17.
A novel co-precipitation and annealing route to the large-quantity synthesis of boron nitride nanotubes (BNNTs), using amorphous boron powder, iron nitrate nonahydrate (Fe(NO3)3·9H2O) and urea (CO(NH2)2) as the raw materials, was demonstrated. An intermediate Fe(OH)3·B was firstly prepared through a co-precipitation process and then annealed in flowing ammonia atmosphere at 1200 °C. It was found that the heat treatment at 800 °C during the annealing process could favor the growth of BNNTs. The BNNTs had an average diameter of 70 nm and possessed bamboo and quasi-cylindrical structures. The annealing temperature greatly affected the formation of BNNTs. Only BN particles could be obtained at lower temperature (e.g. 1100 °C), whereas thorn-like nanosheet-decorated BNNTs were fabricated at higher temperature (e.g. 1300 °C). A combination mechanism of solid–liquid–solid (SLS) and vapor–liquid–solid (VLS) model was suggested to be responsible for the growth of BNNTs.  相似文献   

18.
ZrO2 waveguides are prepared by the sol-gel process from a solution containing zirconiumn-propoxide and acetylacetone in propanol-2. Structural characterizations are investigated for different annealing temperatures using suitable techniques including Waveguide Raman Spectroscopy, Electron Microscopy and Atomic Force Microscopy. Films are amorphous at 300°C and the pure ZrO2 tetragonal crystalline phase appears beyond 400°C. Crystallized films present a dense, uniform and polycrystalline structure made up by randomly oriented nanocrystallites, the diameter of which increases from 38 Å at 400°C to 53 Å at 600°C. Waveguides are at least monomode TE0 at 632.8 nm. At this wavelength, optical losses are about, 0.8±0.2dB/cm for amorphous layers and increase up to 2.5±0.4 dB/cm for 600°C heat-treated waveguides.  相似文献   

19.
Composites containing vitamin B12 (cyanocobalamin) dispersed in amorphous silica xerogel were studied structurally as a function of annealing temperature. Silica xerogel samples were prepared by the sol–gel method using an ethanol:H2O:TEOS molar ratio of 4:11.6:1 and loaded with cyanocobalamin. We found that the structure of the cobalamin is unaltered, although decoordination of the benzimidazole nucleobase of B12, whereas the amorphous quartz structure of the matrix is maintained under heat-treatment without low-cristobalite phase transformation, typically of this kind of materials. We found in our samples partial crystallization of the glass matrix in form of stishovite obtained at very lower pressure than those specified by the phase diagram, and temperatures about 400 °C due to the presence of vitamin B12. The presence of stishovite is corroborated by the Rietveld refinement method.  相似文献   

20.
Sr3(BS3)2 and Sr3(B3S6)2: Two Novel Non‐oxidic Chalcogenoborates with Boron in a Trigonal‐Planar Coordination The thioborates Sr3(BS3)2 and Sr3(B3S6)2 were prepared from strontium sulfide, amorphous boron and sulfur in solid state reactions at a temperature of 1123 K. In a systematic study on the structural cation influence on this type of ternary compounds, the crystal structures were determined by single crystal X‐ray diffraction. Sr3(BS3)2 crystallizes in the monoclinic spacegroup C2/c (No. 15) with a = 10.187(4) Å, b = 6.610(2) Å, c = 15.411(7) Å, β = 102.24(3)° and Z = 4. The crystal structure of Sr3(B3S6)2 is trigonal, spacegroup R3¯ (Nr. 148), with a = 8.605(1) Å, c = 21.542(4) Å and Z = 3. Sr3(BS3)2 contains isolated [BS3]3— anions with boron in a trigonal‐planar coordination. The strontium cations are found between the layers of orthothioborate anions. Sr3(B3S6)2 consists of cyclic [B3S6]3— anions and strontium cations, respectively.  相似文献   

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